CN109437186A - A kind of graphite powder and its denitrification process - Google Patents
A kind of graphite powder and its denitrification process Download PDFInfo
- Publication number
- CN109437186A CN109437186A CN201811405646.2A CN201811405646A CN109437186A CN 109437186 A CN109437186 A CN 109437186A CN 201811405646 A CN201811405646 A CN 201811405646A CN 109437186 A CN109437186 A CN 109437186A
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- China
- Prior art keywords
- graphite powder
- graphite
- denitrification process
- denitrification
- temperature
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
Abstract
The present invention relates to a kind of graphite powder and its denitrification process, the denitrification process includes the following steps: to take graphite powder in graphite boat, the graphite boat is fitted into denitrification equipment, it is vacuumized after being passed through argon gas purging, repeatedly after 1-3 times, continue to be passed through argon gas to the internal pressure of the denitrification equipment to be 1-3KPa；It is warming up to 1500-2000 DEG C, keeps the temperature 1-3h；It is continuously heating to 2200-3000 DEG C, keeps the temperature 3-50h；It is cooled to room temperature, graphite powder is obtained, is vacuum-packed under an argon atmosphere.The present invention can substantially reduce the nitrogen content in graphite powder, and purity also can further improve, and reach the requirement of semiconductor and used in electronic industry graphite powder to nitrogen content and purity.And a kind of denitrification process of graphite powder of the present invention has extremely strong actual promotional value.
Description
Technical field
The present invention relates to graphite composite powder field of material technology, more particularly, to a kind of graphite powder and its denitrification process.
Background technique
On the one hand nitrogen in graphite powder refers to the fixed nitrogen of itself institute's band, such as pyrroles's type nitrogen, pyridine type nitrogen, this kind of nitrogen pole
It is difficult to remove, and on the other hand refers to that the nitrogen adsorbed from air, this kind of nitrogen are all made of simple packet mainly due to current graphite powder
It fills, is just contacted in production process with air, the nitrogen in air can be removed by way of vacuumizing repeatedly subsequent using preceding
Part, but since carbon dust granularity is small, particle inside is mostly uneven, gap is more, but adsorption of nitrogen can not also eliminate.
In recent years, the graphite user of semiconductor and electronics industry proposes graphite specific impurities element very strict
It is required that nitrogen is exactly one of them.In order to meet the needs of semiconductor and electronics industry industry special material, in graphite
The content of nitrogen must be strictly controlled, this just puts forward new requirements the technique of denitrogenating of graphite powder.
Summary of the invention
Based on this, it is necessary to for above-mentioned the technical issues of adsorption of nitrogen not can be removed in the prior art, provide a kind of graphite
Graphite powder purity is increased to 99.9999% or more by 99.99%, nitrogen contains by the denitrification process by powder and its denitrification process
Amount is not more than 2ppm.
In order to solve the above technical problems, the present invention adopts the following technical scheme:
A kind of denitrification process of graphite powder, includes the following steps:
S1, it takes graphite powder in graphite boat, the graphite boat is fitted into denitrification equipment, Xiang Suoshu denitrogenation
It is vacuumized after being passed through argon gas purging in equipment, repeatedly after 1-3 time, continues to be passed through argon gas to internal pressure to be 1-3KPa；
S2, it is warming up to 1500-2000 DEG C, keeps the temperature 1-3h；
S3, it is continuously heating to 2200-3000 DEG C, keeps the temperature 3-50h；
S4, it is cooled to room temperature, the graphite powder is vacuum-packed in the graphite powder after obtaining denitrogenation under an argon atmosphere.
The graphite powder includes in acicular petroleum coke, micro crystal graphite and crystalline flake graphite in one of the embodiments,
It is one or more.
The time for being passed through argon gas purging in one of the embodiments, is 5-10min.
In one of the embodiments, in S2 step, it is warming up to 1800 DEG C.
In one of the embodiments, in S2 step, the rate of heating is 10-15 DEG C/min.
In one of the embodiments, in the S3 step, 2850 DEG C are warming up to.
In one of the embodiments, in the S3 step, the rate of heating is 1-3 DEG C/min.
The present invention also provides a kind of graphite powder, the graphite powder is made by the denitrification process of above-mentioned graphite powder, described
Purity >=99.9999% of graphite powder, nitrogen content are not more than 2ppm.
Denitrification process of the invention destroys internal chemical key using superhigh temperature, separates nitrogen, to eliminate fixed nitrogen；This
Outside, which also uses vacuum and completely cuts off discharging and the packaging system elimination physical absorption nitrogen of air, reaches reduction graphite
The purpose of nitrogen content in powder.Compared with prior art, the present invention can substantially reduce the nitrogen content in graphite powder, and purity is into one
Step improves, and reaches the requirement of semiconductor and used in electronic industry graphite powder to nitrogen content and purity.One kind of the present invention
Graphite powder denitrogenates technique with extremely strong actual promotional value.
Specific embodiment
In the following description, numerous specific details are set forth in order to facilitate a full understanding of the present invention.But the present invention can
Implemented with being much different from other way described herein, those skilled in the art can be without prejudice to intension of the present invention
In the case of do similar improvement, therefore the present invention is not limited to the specific embodiments disclosed below.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff it is identical.Term as used herein in the specification of the present invention is intended merely to retouch
State the purpose of specific embodiment, it is not intended that in the limitation present invention.
Embodiment 1
A kind of denitrification process of graphite powder, includes the following steps:
(1) taking purity is 99.992%, partial size D50 be the petroleum coke 3kg of 0.5~0.8mm be put into having a size of φ 200 ×
In the graphite boat of 150mm, the graphite boat after charging is put into VVN-0308 high temperature of the inner cavity having a size of 300 × 800mm of φ
It in denitrogenation furnace, is passed through after purity >=99.999%Ar carries out purging 10min and vacuumizes, repeatedly after 3 times, filling Ar makes high temperature denitrogenation
Furnace interior pressure is to 1Kpa；
(2) 1800 DEG C are warming up to, 2h, 10 DEG C/min of heating rate are kept the temperature；
(3) 2850 DEG C are warming up to, 20h, 1 DEG C/min of heating rate are kept the temperature；
(4) it is cooled to room temperature, obtains graphite powder, be vacuum-packed under an argon atmosphere.
Through detecting, the nitrogen content of graphite powder made from embodiment 1≤2ppm, purity 99.99992% meets downstream list
The use demand of position.
Embodiment 2
(1) taking purity is 99.995%, and partial size D50 is that the micro crystal graphite 3kg of 0.3~0.5mm is put into having a size of φ 200
In the graphite boat of × 150mm, the graphite boat after charging is put into VVN-0308 high of the inner cavity having a size of 300 × 800mm of φ
It in warm denitrogenation furnace, is passed through after purity >=99.999%Ar carries out purging 10min and vacuumizes, repeatedly after 3 times, filling Ar keeps high temperature de-
Nitrogen furnace interior pressure is 3KPa；
(2) 1850 DEG C are warming up to, 2h, 15 DEG C/min of heating rate are kept the temperature；
(3) 2900 DEG C are warming up to, 25h, 3 DEG C/min of heating rate are kept the temperature；
(4) it is cooled to room temperature, obtains graphite powder, be vacuum-packed under an argon atmosphere.
Through detecting, the nitrogen content of graphite powder made from embodiment 2≤2ppm, purity 99.99994% meets downstream list
The use demand of position.
Embodiment 3
(1) taking purity is 99.993%, and partial size D50 is that the crystalline flake graphite 3kg of 0.2~0.5mm is put into having a size of φ 200
In the graphite boat of × 150mm, the graphite boat after charging is put into VVN-0308 high of the inner cavity having a size of 300 × 800mm of φ
It in warm denitrogenation furnace, is passed through after purity >=99.999%Ar carries out purging 10min and vacuumizes, repeatedly after 3 times, filling Ar keeps high temperature de-
Nitrogen furnace interior pressure is 2KPa；
(2) 1850 DEG C are warming up to, 2h, 13 DEG C/min of heating rate are kept the temperature；
(3) 2850 DEG C are warming up to, 22h, 2 DEG C/min of heating rate are kept the temperature；
(4) it is cooled to room temperature, obtains graphite powder, be vacuum-packed under an argon atmosphere.
Through detecting, the nitrogen content of graphite powder made from embodiment 3≤2ppm, purity 99.99992% meets downstream list
The use demand of position.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (8)
1. a kind of denitrification process of graphite powder, which comprises the steps of:
S1, it takes graphite powder in graphite boat, the graphite boat is fitted into denitrification equipment, in Xiang Suoshu denitrification equipment
It is vacuumized after being passed through argon gas purging, repeatedly after 1-3 time, continues to be passed through argon gas to the internal pressure of the denitrification equipment to be 1-
3KPa；
S2, it is warming up to 1500-2000 DEG C, keeps the temperature 1-3h；
S3, it is continuously heating to 2200-3000 DEG C, keeps the temperature 3-50h；
S4, it is cooled to room temperature, obtains graphite powder, the graphite powder is vacuum-packed under an argon atmosphere.
2. denitrification process according to claim 1, which is characterized in that in S1 step, the graphite powder includes needle
One of shape petroleum coke, micro crystal graphite and crystalline flake graphite are a variety of.
3. denitrification process according to claim 1, which is characterized in that in S1 step, the time for being passed through argon gas purging is
5-10min。
4. denitrification process according to claim 1, which is characterized in that in S2 step, be warming up to 1800 DEG C.
5. denitrification process according to claim 1, which is characterized in that in S2 step, the rate of heating is 10-15 DEG C/
min。
6. denitrification process according to claim 1, which is characterized in that in the S3 step, be warming up to 2850 DEG C.
7. denitrification process according to claim 1, which is characterized in that in the S3 step, the rate of heating is 1-3 DEG C/
min。
8. a kind of graphite powder, which is characterized in that the graphite powder is made by the described in any item denitrification process of claim 1-7,
The purity 99.9999%~99.99999% of the graphite powder, nitrogen content are not more than 2ppm.
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| CN201811405646.2A CN109437186A (en) | 2018-11-23 | 2018-11-23 | A kind of graphite powder and its denitrification process |
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| CN201811405646.2A CN109437186A (en) | 2018-11-23 | 2018-11-23 | A kind of graphite powder and its denitrification process |
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| CN109437186A true CN109437186A (en) | 2019-03-08 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115140729A (en) * | 2022-07-18 | 2022-10-04 | 株洲弗拉德科技有限公司 | Preparation method of high-purity carbon material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2163221C (en) * | 1993-05-21 | 2001-10-30 | Stratmin Inc. | Process and apparatus for the purification of graphite |
| CN105819436A (en) * | 2016-04-28 | 2016-08-03 | 哈尔滨摆渡新材料有限公司 | Method and device for purifying graphite |
| CN106064815A (en) * | 2016-06-01 | 2016-11-02 | 陕西六元碳晶股份有限公司 | The high-purity graphite powder that the method for graphite powder purification and the method are prepared |
| CN207294183U (en) * | 2017-08-24 | 2018-05-01 | 中山国安火炬科技发展有限公司 | A kind of high temperature purification equipment of high-purity carbon nanotubes or graphite powder |
| CN108069422A (en) * | 2017-12-25 | 2018-05-25 | 凯盛石墨碳材料有限公司 | A kind of method of graphite purification |
| CN108675293A (en) * | 2018-07-02 | 2018-10-19 | 凯盛石墨碳材料有限公司 | A kind of graphite high temperature purification device |
-
2018
- 2018-11-23 CN CN201811405646.2A patent/CN109437186A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2163221C (en) * | 1993-05-21 | 2001-10-30 | Stratmin Inc. | Process and apparatus for the purification of graphite |
| CN105819436A (en) * | 2016-04-28 | 2016-08-03 | 哈尔滨摆渡新材料有限公司 | Method and device for purifying graphite |
| CN106064815A (en) * | 2016-06-01 | 2016-11-02 | 陕西六元碳晶股份有限公司 | The high-purity graphite powder that the method for graphite powder purification and the method are prepared |
| CN207294183U (en) * | 2017-08-24 | 2018-05-01 | 中山国安火炬科技发展有限公司 | A kind of high temperature purification equipment of high-purity carbon nanotubes or graphite powder |
| CN108069422A (en) * | 2017-12-25 | 2018-05-25 | 凯盛石墨碳材料有限公司 | A kind of method of graphite purification |
| CN108675293A (en) * | 2018-07-02 | 2018-10-19 | 凯盛石墨碳材料有限公司 | A kind of graphite high temperature purification device |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115140729A (en) * | 2022-07-18 | 2022-10-04 | 株洲弗拉德科技有限公司 | Preparation method of high-purity carbon material |
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